CN111889059A - Reaction device and process for preparing DOTP - Google Patents
Reaction device and process for preparing DOTP Download PDFInfo
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- CN111889059A CN111889059A CN202010890847.7A CN202010890847A CN111889059A CN 111889059 A CN111889059 A CN 111889059A CN 202010890847 A CN202010890847 A CN 202010890847A CN 111889059 A CN111889059 A CN 111889059A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2455—Stationary reactors without moving elements inside provoking a loop type movement of the reactants
- B01J19/2465—Stationary reactors without moving elements inside provoking a loop type movement of the reactants externally, i.e. the mixture leaving the vessel and subsequently re-entering it
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/245—Stationary reactors without moving elements inside placed in series
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/002—Nozzle-type elements
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
Abstract
The invention discloses a reaction device and a process for preparing DOTP, the reaction device comprises a reaction kettle and a submerged jet bypass, and a nozzle is arranged in the upper end of the reaction kettle; an external circulation pipeline is arranged between a liquid outlet at the bottom of the reaction kettle and a nozzle inside the upper end of the reaction kettle, and a circulating pump, a throttling element and a heater are sequentially arranged on the external circulation pipeline; a submerged jet distributor is arranged inside the bottom end of the reaction kettle; one end of the submerging jet bypass is connected to a pipeline between the circulating pump and the throttling element, and the other end of the submerging jet bypass penetrates into the bottom end of the reaction kettle and is connected with the submerging jet distributor. According to the invention, the monoester on the surface of the PTA can be quickly peeled off from the solid surface through the cavitation of the throttling element on the device, and the contact area of the PTA and isooctanol is increased in the reaction process, so that the reaction rate is increased, and the energy consumption is reduced; in addition, the method can be used for carrying out intermittent operation of a single kettle and continuous operation of a plurality of kettles connected in series to carry out reaction synthesis of DOTP.
Description
Technical Field
The invention belongs to the technical field of liquid-solid heterogeneous reaction, and particularly relates to a reaction device and a process for preparing DOTP.
Background
The traditional o-benzene plasticizer is most widely applied as DOP, but has potential carcinogenic and teratogenic risks, is an environmental estrogen, and is limited by relevant policies in countries such as Europe and America at present. DOTP (for preparing DOTP) is an effective substitute of DOP, is widely applied to PVC products and has excellent plasticizing performance. At present, the liquid-solid heterogeneous esterification reaction is carried out by a stirring device in the industry, and the problems of low reaction rate and high energy consumption exist. Different approaches have been proposed to address the existing problems.
Chinese patent CN 102952019 proposes a dioctyl phthalate production line and a DOTP production and preparation method, the dioctyl terephthalate production line comprises an esterification system, a dealcoholization system, a neutralization/water washing system, a stripping system, a filtering and decoloring system and a sewage purification and recovery system which are modified, the esterification reaction can be completed within 4-5 hours, the catalyst dosage is small, the product is clean and colorless, the alcohol content in the finished product can be reduced to 20ppm, and the quality is greatly improved. Chinese patent CN 105130804 proposes a production method and a production system for preparing DOTP by an environment-friendly plasticizer, wet materials are fed into a double-helix meter and added with octanol for mixing and presoaking, then the wet materials are fed into an esterification kettle, added with alkali solution for stirring and washing, the PH value is controlled to be neutral, and the temperature is raised to evaporate water; continuously feeding materials by utilizing the vacuum action; a decoloring agent is added to improve the decoloring effect; heating under the action of vacuum, adding diatomite and kaolin into the filter, and filtering to obtain the product. Chinese patent CN 204897793 provides a plasticizer esterification reaction device for preparing DOTP, which comprises an esterification kettle, a buffer tank, an esterification kettle, an esterification tower, a condenser, an alcohol-water separation tank, a water discharge solenoid valve, a secondary sedimentation separation tank and a neutralization water washing tank which are connected in sequence, wherein the top of the esterification kettle is connected with a feed inlet through a feed valve, the esterification tower, a U-shaped pipe and the alcohol-water separation tank are connected in sequence, and an interface meter is arranged on the alcohol-water separation tank. Chinese patent CN 204589035 proposes an esterification pressure reaction system for preparing DOTP, which can significantly increase the reaction temperature and reduce the volatilization of octanol by adjusting the reaction pressure in the early stage of the reaction through an adjusting valve, and simultaneously, the excessive alcohol at the bottom of the esterification tower is continuously injected into the esterification kettle, thereby increasing the esterification reaction rate and reducing the reaction time.
However, the reaction apparatuses used in the above production methods are all stirring apparatuses, and the rotation speed of the stirring apparatuses in industry is usually 50-150 rpm, and the disturbance generated by rotation is not enough to rapidly peel off the monoester generated on the surface of PTA, and the contact area of PTA and isooctanol is prevented, so that the reaction rate is reduced and the energy consumption is increased. Therefore, there is still a need for improvement in the apparatus structure of the reaction tank.
Disclosure of Invention
In order to solve the technical problems in the prior art, the present application aims to provide a reaction device and a process for preparing DOTP.
The reaction device for preparing DOTP is characterized by comprising a reaction kettle and a submerged jet bypass, wherein a nozzle is arranged inside the upper end of the reaction kettle; an external circulation pipeline is arranged between a liquid outlet at the bottom of the reaction kettle and a nozzle inside the upper end of the reaction kettle, and a circulating pump, a throttling element and a heater are sequentially arranged on the external circulation pipeline; a submerged jet distributor is arranged inside the bottom end of the reaction kettle; one end of the submerged jet bypass is connected to a pipeline between the circulating pump and the throttling element, and the other end of the submerged jet bypass penetrates into the bottom end of the reaction kettle and is connected with the submerged jet distributor; the reaction mixed liquid flowing out of the bottom of the reaction kettle is pumped out by two paths through a circulating pump, one path is heated through a heater after cavitation is realized through a throttling element, and then is sprayed into the reaction kettle again through a nozzle; the other path enters the submerged jet distributor through the submerged jet bypass and is sprayed into the bottom of the reaction kettle by the submerged jet distributor.
The reaction device for preparing DOTP is characterized in that a heat recovery circulating system is connected to a reaction kettle, and the heat recovery circulating system comprises a packed tower, a condenser and a water distribution tank; the top gas lifting port of the packed tower is connected with the water distribution tank through a condenser by a pipeline, a liquid outlet at the upper part of the water distribution tank is connected with a reflux port at the top of the packed tower by a pipeline, and a liquid outlet at the bottom of the water distribution tank is used for discharging separated liquid water; an air inlet at the lower part of the packed tower is connected with an air outlet at the top of the reaction kettle through a pipeline, and a liquid outlet at the bottom of the packed tower is connected with a liquid inlet at the side part of the reaction kettle through a pipeline.
The reaction device for preparing DOTP is characterized in that the throttling element is a Venturi tube, an orifice plate, a valve or a reducer pipe.
A reaction process for preparing DOTP based on the reaction device is characterized by comprising the following steps: firstly, adding PTA solid powder and isooctanol into a reaction kettle respectively, starting a circulating pump, pumping out reaction mixed liquid flowing out of the bottom of the reaction kettle by the circulating pump in two paths, preheating the reaction mixed liquid by a heater after cavitation of one path is realized by a throttling element, and then spraying the reaction mixed liquid into the reaction kettle again by a nozzle to form an external circulation loop of the reaction mixed liquid; the other path of the PTA solid enters the submerged jet distributor through the submerged jet bypass and is sprayed into the bottom of the reaction kettle by the submerged jet distributor to prevent the PTA solid from settling down in the bottom of the reaction kettle; when the temperature of the reaction mixed liquid in the reaction kettle is heated to the reaction temperature, a titanate catalyst is added, so that the reaction mixed liquid circularly flows between the reaction kettle and an external circulation pipeline, and reacts to synthesize DOTP under the condition that the reaction mixed liquid is cavitated.
The reaction process for preparing DOTP is characterized in that when the reaction mixed liquid circularly flows between the reaction kettle and the external circulation pipeline, the pressure of the reaction mixed liquid flowing through the inlet of the throttling element is 0.1-2 Mpa.
The reaction process for preparing DOTP is characterized in that the reaction kettle is operated at normal pressure, and the reaction temperature is 180-240 ℃.
The reaction process for preparing DOTP is characterized in that a pipeline between a throttling element and a nozzle is marked as a main pipeline; when the reaction mixed liquid is pumped out in two ways by the circulating pump, the ratio of the flow rate of the reaction mixed liquid flowing through the main pipeline to the flow rate of the reaction mixed liquid in the submerged jet bypass is 1: 0.01-1: 0.2.
The reaction process for preparing DOTP is characterized in that the titanate catalyst is tetrabutyl titanate or isopropyl titanate.
The reaction process for preparing DOTP is characterized in that a single reaction kettle is adopted to carry out intermittent production operation in the process of preparing DOTP, or at least 2 stages of reaction kettles which are sequentially connected in series are adopted to realize continuous production operation.
Wherein, the molecular chain of terephthalic acid (PTA) contains two carboxyl groups. When PTA and isooctyl alcohol react under the action of a catalyst, the process mechanism of the reaction is as follows: a carboxyl in a PTA molecular chain reacts with an isooctanol molecule to generate liquid monoester, and the monoester molecular chain contains a carboxyl and an ester group, so that the monoester molecule has certain amphipathy, namely the carboxyl of the monoester molecule has stronger affinity with the PTA, and the ester group of the monoester molecule has stronger compatibility with the isooctanol. Thus, the monoester produced is easily adhered to the surface of the solid PTA, and the solid PTA is prevented from further contact reaction with isooctanol molecules. In addition, the monoester molecule produced in the first step is subjected to the second step reaction, and is continuously contacted with isooctanol to produce Diester (DOTP). However, since the carboxyl terminal of the monoester is easily adhered to the surface of the solid PTA, the carboxyl of the monoester is not released to be in contact with isooctanol, and the process of generating the diester through the second step reaction is also affected in a certain negative way.
In the production process, the reaction mixed liquor circularly flows between the reaction kettle and the external circulation pipeline, the reaction mixed liquor generates cavitation after passing through the throttling element, the cavitated liquid phase material impacts the surface of the PTA solid powder at a high speed, and the monoester is rapidly stripped from the surface of the PTA under the action of high impact, so that the updating of the surface of the PTA solid is promoted, the surface of the PTA solid can realize good contact reaction with the isooctanol raw material, and the reaction rate is increased.
By adopting the technology, compared with the prior art, the invention has the following beneficial effects:
1. the reaction device can ensure that the PTA particles are uniformly distributed through the nozzle on the circulating pipeline and the submerged jet device, thereby avoiding the problem of incomplete esterification caused by the deposition of the PTA particles at the bottom of the kettle; the water generated by the reaction can be timely analyzed out of the system by spraying through a circulating pipeline nozzle, and the reaction rate is improved.
2. In the reaction device, the throttling element is arranged on the external circulation pipeline of the reaction kettle, and the monoester adhered to the surface of the PTA can be quickly stripped from the solid surface through the cavitation action of the throttling element on the pipeline, so that the contact area of the PTA and isooctanol is increased in the reaction process, the reaction rate is further improved, and the energy consumption is reduced; in addition, the reaction device of the invention can use a single reaction kettle to carry out batch operation, and can also use a plurality of kettles connected in series to realize continuous operation.
Drawings
FIG. 1 is a schematic structural view of a reaction apparatus for preparing DOTP according to the present invention;
in fig. 1: 1-a heater, 2-a throttling element, 3-a circulating pump, 4-a nozzle, 5-a liquid outlet, 6-a reaction kettle, 7-a packed tower, 8-a condenser and 9-a water diversion tank;
FIG. 2 is a process flow chart of a third embodiment of the present invention in which three stages of reaction vessels are connected in series to achieve continuous production operation.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example (b):
the reaction device comprises a reaction kettle 6, wherein a nozzle 4 is arranged inside the upper end of the reaction kettle 6; an external circulation pipeline is arranged between a liquid outlet at the bottom of the reaction kettle 6 and a nozzle 4 inside the upper end of the reaction kettle 6, and a circulation pump 3, a throttling element 2 and a heater 1 are sequentially arranged on the external circulation pipeline. Referring to fig. 1, a liquid outlet 5 is further arranged at the bottom of the reaction kettle 6.
Referring to fig. 1, the reaction apparatus of the present invention further comprises a submerged jet bypass, and a corresponding submerged jet distributor is disposed inside the bottom end of the reaction vessel 6; one end of the submerged jet bypass is connected to a pipeline between the circulating pump 3 and the throttling element 2, and the other end of the submerged jet bypass penetrates into the bottom end of the reaction kettle 6 and is connected with the submerged jet distributor. When the device works, reaction mixed liquid flowing out of the bottom of the reaction kettle 6 is pumped out in two ways by the circulating pump 3, and after cavitation is realized on one way by the throttling element 2, the reaction mixed liquid is heated by the heater 1 and then is sprayed into the reaction kettle 6 again by the nozzle 4; the other path enters the submerged jet distributor through a submerged jet bypass, and the submerged jet distributor sprays reaction mixed liquid to the inside of the bottom end of the reaction kettle 6.
Further, the reaction kettle 6 is connected with a heat recovery circulating system, and the heat recovery circulating system comprises a packed tower 7, a condenser 8 and a water distribution tank 9; an air lifting port at the top of the packed tower 7 is connected with a water distribution tank 9 through a condenser 8 by a pipeline, a liquid outlet at the upper part of the water distribution tank 9 is connected with a reflux port at the top of the packed tower 7 by a pipeline, and a liquid outlet at the bottom of the water distribution tank 9 is used for discharging separated liquid water; an air inlet at the lower part of the packed tower 7 is connected with an air outlet at the top of the reaction kettle 6 through a pipeline, and a liquid outlet at the bottom of the packed tower 7 is connected with a liquid inlet at the side part of the reaction kettle 6 through a pipeline.
In the process of preparing DOTP, the heat recovery circulation system has the following functions:
1. mixing steam of unreacted isooctanol and byproduct water is continuously evaporated from the reaction kettle 6, the mixing steam is introduced into the packed tower 7 from an air inlet at the lower part of the packed tower 7 in a gas phase feeding mode, the mixing steam continuously rises in the packed tower 7 and finally flows out from an air lifting port at the top of the packed tower 7, and enters the water diversion tank 9 for layered dewatering after being condensed by the condenser 8, a liquid outlet at the bottom of the water diversion tank 9 discharges separated liquid water, and a liquid outlet at the upper part of the water diversion tank 9 discharges dewatered liquid isooctanol raw material;
2. the dehydrated liquid isooctanol raw material is introduced into the packed tower 7 from a reflux port at the top of the packed tower 7 in a reflux mode, the liquid isooctanol raw material is in reverse contact with ascending mixed steam in the process of flowing downwards in the packed tower 7 to carry out heat and mass transfer, and the liquid flowing out from a liquid outlet at the bottom of the packed tower 7 finally reflows to the reaction kettle 6 again to carry out reaction.
The restriction element 2 may be a venturi tube, an orifice plate, a valve or a reducer. In the following examples two and three, the throttling element of the reaction apparatus employed was a venturi tube.
When the device of this application is utilized to prepare DOTP, can use single reation kettle intermittent type operation, also can multistage reation kettle establishes ties and realize serialization production operation.
The first embodiment is as follows:
DOTP was prepared in batch mode using a conventional stirring apparatus:
adding PTA solid powder and isooctanol into a reaction kettle, wherein the feeding molar ratio of the PTA solid powder to the isooctanol is 1: 3, mechanically stirring (stirring speed is 400 rpm), preheating the reaction materials to 180 ℃, adding tetrabutyl titanate catalyst, wherein the dosage of the catalyst is 0.4 percent of the weight of the PTA, and marking the reaction as the beginning of the reaction. During the reaction, the temperature of the system is gradually increased, and the reaction is considered to be complete when the reaction temperature reaches 225 ℃ (the PTA conversion rate is nearly 100%), and the reaction time is 5 hours in total.
Example two:
the production of DOTP was carried out in batch operation using a reaction apparatus as shown in fig. 1:
adding PTA solid powder and isooctyl alcohol into a reaction kettle, wherein the feeding molar ratio of the PTA solid powder to the isooctyl alcohol is 1: 3. starting a circulating pump, pumping out reaction mixed liquid flowing out of the bottom of the reaction kettle in two ways by the circulating pump, heating the reaction mixed liquid by a heater after cavitation is realized by a throttling element in one way, and spraying the reaction mixed liquid into the reaction kettle again by a nozzle; the other path of the jet flow enters the submerged jet flow distributor through the submerged jet flow bypass and is sprayed into the bottom end of the reaction kettle by the submerged jet flow distributor. The reaction kettle is operated under normal pressure, the inlet pressure of the throttling element is controlled to be 2.5 bar, and the ratio of the flow rate of the reaction mixed liquid flowing into the main pipeline of the throttling element to the flow rate of the reaction mixed liquid flowing through the submerged jet bypass is 1: 0.1.
After preheating the reaction mass to 180 ℃, tetrabutyl titanate catalyst was added in an amount of 0.4% by weight of PTA, which was recorded as the start of the reaction. During the reaction, the temperature of the system is gradually increased, and the reaction is considered to be complete when the reaction temperature reaches 225 ℃ (the PTA conversion rate is nearly 100%), and the reaction time is 2 hours in total.
Example three:
in the third embodiment, when preparing DOTP, the reaction apparatus uses three stages of reaction kettles connected in series to realize continuous production operation, each stage of reaction kettle uses a single kettle apparatus as shown in fig. 1, and the process flow of the three stages of reaction kettles connected in series to realize continuous production operation is shown in fig. 2.
The continuous production process comprises the following steps:
adding PTA solid powder and isooctyl alcohol into a first-stage reaction kettle, wherein the feeding molar ratio of the PTA solid powder to the isooctyl alcohol is 1: 2. And starting the circulating pump, pumping out the reaction mixed liquid flowing out of the bottom of the first-stage reaction kettle in two ways by the circulating pump, and respectively returning the reaction mixed liquid into the first-stage reaction kettle again. Preheating the reaction material to 180 ℃, and then adding tetrabutyl titanate catalyst, wherein the dosage of the catalyst is 0.4% of the weight of PTA; at which point the reaction begins. Allowing the reaction material containing the catalyst to stay in the first-stage reaction kettle for 1h, then allowing the reaction material to enter a second-stage reaction kettle, and supplementing 0.5 molar percent of octanol into the second-stage reaction kettle (namely, the ratio of the supplemented octanol to the PTA raw material added into the first-stage reaction kettle is 0.5:1, the same applies below); the reaction material containing the catalyst enters a third-stage reaction kettle after staying in the second-stage reaction kettle for 0.5h, 0.5 mol proportion of octanol is added into the third-stage reaction kettle, the reaction is considered to be complete when the reaction temperature of the third-stage reaction kettle reaches 225 ℃ (the PTA conversion rate is nearly 100 percent at this moment), and the staying time of all the reaction kettles is 2 h in total.
Wherein, the control process of the first-stage, the second-stage and the third-stage reaction kettles is as follows: the reaction kettle is operated under normal pressure, the inlet pressure of the throttling element is controlled to be 2.5 bar, and the ratio of the flow rate of the reaction mixed liquid flowing into the main pipeline of the throttling element to the flow rate of the reaction mixed liquid flowing through the submerged jet bypass is 1: 0.1.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (9)
1. A reaction device for preparing DOTP is characterized by comprising a reaction kettle (6) and a submerged jet bypass, wherein a nozzle (4) is arranged inside the upper end of the reaction kettle (6); an external circulation pipeline is arranged between a liquid outlet at the bottom of the reaction kettle (6) and a nozzle (4) inside the upper end of the reaction kettle (6), and a circulating pump (3), a throttling element (2) and a heater (1) are sequentially arranged on the external circulation pipeline; a submerged jet distributor is arranged inside the bottom end of the reaction kettle (6); one end of the submerged jet bypass is connected to a pipeline between the circulating pump (3) and the throttling element (2), and the other end of the submerged jet bypass penetrates into the bottom end of the reaction kettle (6) and is connected with the submerged jet distributor;
the reaction mixed liquid flowing out of the bottom of the reaction kettle (6) is pumped out by two paths through a circulating pump (3), and after cavitation is realized on one path through a throttling element (2), the reaction mixed liquid is heated through a heater (1), and then is sprayed into the reaction kettle (6) again through a nozzle (4); the other path enters the submerged jet distributor through a submerged jet bypass and is sprayed into the bottom of the reaction kettle (6) by the submerged jet distributor.
2. A reaction unit for preparing DOTP according to claim 1, wherein the reaction vessel (6) is connected to a heat recovery circulation system comprising a packed tower (7), a condenser (8) and a water knockout drum (9); a gas lifting port at the top of the packed tower (7) is connected with a water distribution tank (9) through a condenser (8) by a pipeline, a liquid outlet at the upper part of the water distribution tank (9) is connected with a reflux port at the top of the packed tower (7) by a pipeline, and a liquid outlet at the bottom of the water distribution tank (9) is used for discharging separated liquid water; an air inlet at the lower part of the packed tower (7) is connected with an air outlet at the top of the reaction kettle (6) through a pipeline, and a liquid outlet at the bottom of the packed tower (7) is connected with a liquid inlet at the side part of the reaction kettle (6) through a pipeline.
3. A reaction unit for the preparation of DOTP according to claim 1, characterized in that the throttling element (2) is a venturi tube, an orifice plate, a valve or a reducer.
4. A reaction process for preparing DOTP based on the reaction device of claim 1, which is characterized in that the process comprises the following steps: firstly, adding PTA solid powder and isooctanol into a reaction kettle (6) respectively, starting a circulating pump (3), pumping out reaction mixed liquid flowing out of the bottom of the reaction kettle (6) by the circulating pump (3) in two ways, preheating by a heater (1) after cavitation of one way of the reaction mixed liquid is realized by a throttling element (2), and then spraying the reaction mixed liquid into the reaction kettle (6) again by a nozzle (4) to form an external circulation loop of the reaction mixed liquid; the other path of the PTA solid enters the submerged jet distributor through a submerged jet bypass and is sprayed into the bottom of the reaction kettle (6) by the submerged jet distributor to prevent the PTA solid from settling in the bottom of the reaction kettle (6);
when the temperature of the reaction mixed liquid in the reaction kettle (6) is heated to the reaction temperature, the titanate catalyst is added, so that the reaction mixed liquid generates circulation flow between the reaction kettle (6) and an external circulation pipeline, and reacts to synthesize DOTP under the condition of cavitation of the reaction mixed liquid.
5. A DOTP production process in accordance with claim 4 wherein the inlet pressure of the reaction mixture through the throttling element (2) is 0.1-2 MPa when the reaction mixture is circulated between the reactor (6) and its external circulation line.
6. A reaction process for the preparation of DOTP according to claim 4, characterized in that the reaction vessel (6) is operated at atmospheric pressure and the reaction temperature is 180-240 ℃.
7. A DOTP production reaction process as claimed in claim 4 wherein the line between the throttling element (2) and the nozzle (4) is marked as the main conduit; when the reaction mixed liquid is pumped out in two ways by the circulating pump (3), the ratio of the flow of the reaction mixed liquid flowing through the main pipeline to the flow of the reaction mixed liquid in the submerged jet bypass is 1: 0.01-1: 0.2.
8. A DOTP according to claim 4 wherein the titanate-based catalyst is tetrabutyl titanate or isopropyl titanate.
9. A DOTP production process as claimed in claim 1 wherein the DOTP production process uses a single reactor (6) for batch production operations or at least 2 reactors (6) connected in series in sequence for continuous production operations.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112679345A (en) * | 2020-12-30 | 2021-04-20 | 南京中设石化工程有限公司 | Method for preparing environment-friendly plasticizer by continuous esterification method |
| CN113318677A (en) * | 2021-05-18 | 2021-08-31 | 浙江工业大学 | DOTP production device and process |
| CN114768278A (en) * | 2022-04-07 | 2022-07-22 | 浙江工业大学 | Energy-saving efficient DOTP continuous production device and production process thereof |
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